Methyl chloroacetate → HCID 19963012、化合物

HRID 52149ノート

反応式

HRID 52149 の反応式
[CH3:1][C:2]1[C:3]([CH2:19][S:20][C:21]2[NH:25][C:24]3[CH:26]=[CH:27][CH:28]=[CH:29][C:23]=3[N:22]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][NH:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.Cl[CH2:31][C:32]([O:34][CH3:35])=[O:33].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:1][C:2]1[C:3]([CH2:19][S:20][C:21]2[NH:22][C:23]3[CH:29]=[CH:28][CH:27]=[CH:26][C:24]=3[N:25]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:8][CH2:9][CH2:10][N:11]([CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:31][C:32]([O:34][CH3:35])=[O:33]

参加物

5

反応物 3

HCID 7295Methyl chloroacetateHCID 11430Potassium CarbonateHCID 199630842-((3-Methyl-4-(2-benzylaminoethylthio)pyridin-2-yl)methylthio)-1H-benzimidazole

生成物 1

HCID 19963012HCID 19963012、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-((3-Methyl-4-(2-benzylaminoethylthio)pyridin-2-yl)methylthio)-1H-benzimidazole (2 g) was dissolved in dimethylformamide and reacted with methyl chloroacetate (0.45 ml) in the presence of potassium carbonate (0.71 g) at 50°-60° C. After the completion of the reaction, the dimethylformamide was distilled away and the residue was extracted with ethyl acetate. The ethyl acetate layer was dried over anhydrous magnesium sulfate and the solvent was distilled away to give an oily product. The oily product was purified by column chromatography to give 2-((3-methyl-4-(2-(N-benzyl-N-methoxycarbonylmethylamino)ethylthio)-2-pyridyl)methylthio)-1H-benzimidazole.

後処理

  1. customAfter the completion of the reaction
  2. distillationthe dimethylformamide was distilled away
  3. extractionthe residue was extracted with ethyl acetate
  4. dry with materialThe ethyl acetate layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled away
  6. customto give an oily product
  7. customThe oily product was purified by column chromatography

出典と根拠

ORDレコード
ord-358770dc8b62426c8b8107acc0b2f1eb
出典データセット
uspto-grants-1997_04
特許番号
US05616581

反応ノート

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